EP0469014B1 - Emulsion liquide sans emulsifiant; procede et dispositif pour la preparer - Google Patents

Emulsion liquide sans emulsifiant; procede et dispositif pour la preparer Download PDF

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Publication number
EP0469014B1
EP0469014B1 EP90906170A EP90906170A EP0469014B1 EP 0469014 B1 EP0469014 B1 EP 0469014B1 EP 90906170 A EP90906170 A EP 90906170A EP 90906170 A EP90906170 A EP 90906170A EP 0469014 B1 EP0469014 B1 EP 0469014B1
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EP
European Patent Office
Prior art keywords
mixture
chamber
flow
emulsion
axis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP90906170A
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German (de)
English (en)
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EP0469014A1 (fr
Inventor
Armando Ulrich
Walter H. Ott
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tecno-Bio Co Ltd
Original Assignee
Tecno-Bio Co Ltd
Techno Bio Co Ltd
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Publication date
Priority claimed from DE8905075U external-priority patent/DE8905075U1/de
Application filed by Tecno-Bio Co Ltd, Techno Bio Co Ltd filed Critical Tecno-Bio Co Ltd
Publication of EP0469014A1 publication Critical patent/EP0469014A1/fr
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Publication of EP0469014B1 publication Critical patent/EP0469014B1/fr
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/41—Emulsifying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/10—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/10—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components
    • B01F25/102—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components wherein the vortex is created by two or more jets introduced tangentially in separate mixing chambers or consecutively in the same mixing chamber
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F2025/91—Direction of flow or arrangement of feed and discharge openings
    • B01F2025/919—Direction of flow or arrangement of feed and discharge openings characterised by the disposition of the feed and discharge openings
    • B01F2025/9191—Direction of flow or arrangement of feed and discharge openings characterised by the disposition of the feed and discharge openings characterised by the arrangement of the feed openings for one or more flows, e.g. for the mainflow and the flow of an additional component

Definitions

  • the present invention relates to a method and a device for producing an emulgator-free liquid emulsion of at least one hydrophobic phase and at least one hydrophilic phase.
  • GB-A-2 092 025 discloses a method of forming and spraying emulsions of two immiscible liquids by introducing small amounts of a first liquid into a body of a second liquid while electrically charging the first liquid relative to the second liquid to a potential sufficient to cause emulsification therein, and atomising the charged emulsion thereby formed. Atomising the emulsion immediately after mixing results in reducing or eliminating storage time, thereby preventing emulsion break-down.
  • FR-A-844009 discloses a method for preparing emulsions and colloidal suspensions of vaseline oil, perfume, aromatic essences or the like in water by using ultrasonic in order to obtain very fine emulsions with a particle size of less than 0.4 ⁇ m.
  • AU-A-541324 discloses a method for preparing emulsions of immiscible fluids, e.g. oil in water, of a particle size from 0.1 to more than 50 ⁇ m by passing the mixture through a column packed with steel metal sponge, animal hair or plastic brush or the like in the presence of an emulsifier, e.g. Sapotin.
  • EP-A-0 263 443 discloses an apparatus for preparing a water-in-oil-emulsion comprising a mixing apparatus according to the introduction portion of claim 3 in a recirculation conduit path.
  • a storage container is connected in the recirculation conduit path behind the mixing apparatus, the emulsion being held in continuous movement in the storage container in order to avoid a decomposition of the mixture.
  • Another object of the present invention is to provide a mixing device for use in carrying out this mixing method.
  • Still another object of the present invention is to provide a stable emulsion of at least one hydrophobic liquid phase and at least one hydrophilic liquid phase and prepared or preparable by this mixing apparatus.
  • the emulgator-free emulsion, the method and the mixing device in accordance with the present invention have especially the features as described in the claims.
  • a colloidal emulgator-free emulsion comprising a hydrophilic liquid, especially water, and a hydrophobic liquid, wherein fine liquid drops of the disperse liquid phase are homogeneously and stably distributed in the emulsion without the aid of an emulsifier.
  • the preferred composition of the water/hydrophobic liquid mixture is such that the amount of the hydrophobic liquid is up to 20% by volume based on water.
  • a mixture comprising water and a hydrophobic liquid, wherein fine liquid drops of the water are homogeneously and stably distributed in the hydrophobic liquid without the aid of an emulsifier.
  • the preferred composition of the water/hydrophobic liquid mixture is such that the amount of the water is 5-35% by volume based on the hydrophobic liquid.
  • a colloidal mixture comprising a hydrophilic liquid and a hydrophobic liquid, wherein fine liquid drops are homogeneously and stably distributed without the aid of an emulsifier.
  • the preferred composition of the hydrophilic liquid and the hydrophobic liquid is such that the amount of the hydrophobic liquid is up to 20% by volume based on the hydrophilic liquid.
  • colloidal state means a state in which colloidal particles having a size of about 1,000 nm or less are contained, the existence of the colloidal particles and the occurrence of a Brownian movement are confirmed by an ultramicroscope, and a Tyndall phenomenon is observed.
  • Fig. 1 is a diagram illustrating a general layout of a preferred first embodiment of the mixing device comprising a mixing apparatus used in the present invention.
  • Fig. 2 is an elevation sectional view of the mixing apparatus 1 shown in Fig. 1.
  • Fig. 3 is a cross sectional view or the top portion of the mixing apparatus 1 shown in Fig. 1.
  • Fig. 4 is a diagram illustrating a second embodiment of the mixing device used in the present invention.
  • Fig. 5 is a diagram illustrating a third embodiment of the mixing device used in the present invention .
  • Fig. 6 is a diagram illustrating the structure of an example of the cylindrical housing defining the hollow interior space of the jet pump 50 of the mixing device shown in Fig. 5.
  • FIG. 1 A general device according to the first embodiment of the device for use in carrying out the present invention is shown in Fig. 1.
  • the elevation of a mixing apparatus 1 is shown in Fig. 2 and the top section of the mixing apparatus 1 in the plane of a hole of the mixing apparatus 1 is shown in Fig. 3.
  • the mixing apparatus 1 is described with reference to Figs. 2 and 3.
  • the mixing apparatus 1 comprises a cylindrical wall which is opened at one end 10 and closed at the opposite end 11.
  • a hollow element 13 comprising a first portion 14 having a circular rim 12 connected to the central part thereof and a second portion 17.
  • the first portion 14 of this element 13 has a shape of a substantially hollow parabolic surface arranged in a closed chamber formed between the rim 12 and the closed end 11 of the mixing apparatus 1.
  • the first portion 14 has a shape of a completely hollow parabolic surface.
  • a certain number of holes 15 are formed through wall of the element 13 at the height (about 1/3 in the embodiment) of the upper position of the first portion 14. The holes 15 are formed in the tangential direction.
  • a duct 16 is extended from the closed end 11 of the mixing apparatus 1 slightly inclinedly with respect to the axis of the mixing apparatus.
  • the element 13 includes the second portion 17 communicating with the first portion 14 at the plane of the rim 12, and this portion has a substantially tapered shape which is continuous as a short cylindrical duct 18.
  • the portion 17 has a shape of a complete hyperbola.
  • the mixing apparatus 1 is formed of glass.
  • a fluid component is caused to flow to the first portion 14 through the inclined duct 16 while being rotated, and in the first portion 14, the majority of the fluid component introduced into the holes 15 is caused to flow along the inner wall of the fist portion 14 toward the top (downward in Fig. 2) while being further rotated. At the top, the flow is reflected and the flow speed is gradually increased, and a vortex state is formed on the central axis toward the second portion. Different substances are mixed by this vortex state.
  • a liquid mixture of a hydrophobic liquid phase and an hydrophilic liquid phase is introduced through the inlet duct 16.
  • the inflowing fluid will rotate around the central axis of the mixing apparatus 1 and the rotating fluid enters in through the tangential openings 15 in the wall 14 of the first chamber portion.
  • a focal line is formed where pressure is at minimum, and along the axis the pressure decreases in axial direction towards the outlet opening. This means that pressure is decreasing gradually both in radial and axial direction, and the fluid rotates around the axis and flows in axial direction.
  • the speed of flow and the velocity of rotation increases gradually toward the outlet duct portion 18 and in radial direction the pressure decreases towards the axis and a minimum is experienced along the axis. It is preferred if the rotational hyperboloid function has the same grade as the paraboloid function of the first chamber portion has.
  • the flow will have a structure which can be visualized in such a way as if the fluid mass consisted of an infinitely high numbers of annular hollow tubes having a form substantially following that of the tapering section 17, and the speed of rotation was different in case of each tube so that the elementary tubes were sliding on each other during their rotational movements. Moreover, the elementary tubes slide with respect to each other not only due to their differing speeds of rotation but they are moving and sliding in axial direction as well.
  • the flow rate should be adjusted in such a way that phase transition (i.e. vaporization of any component) do not take place, nevertheless the minimum pressure should be just above the vapour pressure of the liquid mixture.
  • this condition should relate to the one which has the highest vapor pressure at the given temperature.
  • This condition is equivalent to the statement that cavitation cannot occur in the flow.
  • the mixing apparatus being preferably of glass, said condition can be adjusted by increasing the flow velocity up to a measure at which fine gas bubbles appear in the duct portion 18, and then lowering the flow velocitity by a small amount just until the gas bubbles dissappear again.
  • a closed circulation passage comprising a pump 2 and a vessel 3, which are connected to each other through conduits 4, 5, 6 and 7, is formed.
  • Reference numeral 8 represents a withdrawal opening for the withdrawal of a mixture, which has a cock. The opening is always closed except at the time of the withdrawal of the mixture.
  • the vessel 3 has a cock-provided duct 31 and a cock-provided duct 32 for charging starting materials to be formed into a mixture. The fluid flows as indicated by arrows.
  • the cock of the duct 31 is opened and 9 l of distilled water is filled in the vessel 3. Then, the cock of the duct 3Z is opened and 1 l of a vitamin A oil as the starting oil is filled in the vessel 3 and the cocks of the ducts 31 and 32 are closed.
  • the vessel 3 is fully filled with water and vitamin A oil, or the upper portion of the vessel 3 may be vacant.
  • the pump 2 is started.
  • This pump has a flow quantity of 25 l/min.
  • the inner diameters of the conduits 4, 5, 6 and 7 are equally about 14 mm.
  • the flow direction is indicated by arrows in Fig. 1.
  • Water and vitamin A oil are introduced into the mixing apparatus 1, and in the mixing apparatus 1, water and vitamin A oil flow into the interior of the cylindrical wall from the inclined duct 16 while being rotated and flow in the first portion 14 through the tangential holes 15 to form a vortex in the hollow element 13. This will now be described in detail.
  • the majority of the rotating fluid component first flows to the closed top of the paraboloid and is reflected forward therefrom, and because of the exponentially tapered shape of the second portion 17 of the hollow element 13, the fluid component is promptly rotated together with the other component and the fluid component is advanced in the conduit 5 toward the vessel 3.
  • the fluid component is circulated in the closed system until the pump 2 is turned off.
  • the cock is opened and the water/vitamin A oil mixture is withdrawn from the withdrawal opening 8.
  • a hydrophilic liquid is mixed with a hydrophobic liquid by using the mixing device of the embodiment shown in Fig. 1
  • the cock of the duct 31 is opened, and the vessel 3 is filled with 9 l of ethyl alcohol, and then the cock of the duct 32 is opened and 1 l of of a vitamin oil is filled in the vessel 3.
  • the subsequent procedures are the same as described above.
  • a mixture of 9 l of a vitamin A oil and 1 l of ethyl alcohol is similarly prepared according to the above-mentioned method.
  • the obtained mixture formed by mixing ethyl alcohol and vitamin A oil without the aid of an emulsified according to the above-mentioned method can be widely used for cosmetic lotions and cosmetic creams.
  • the second embodiment is different from the first embodiment mainly in that a vessel 9 for forming a second vortex is used instead of the mixing apparatus 3.
  • the vessel 9 has a substantially spherical upper part 91, a lower part 93 tapered downwardly and an intermediate part 92 connected smoothly to the spherical upper part 91 and the lower part 93.
  • the upper part 91 and intermediate part 92 have a convex face and the lower part 93 has a concave face.
  • an inflection face is formed between the intermediate part 92 and the lower part 93.
  • the vessel 9 is formed of glass so that the process occurring in the vessel 9 can be observed.
  • Three ducts 95, 96 and 97 are formed on the top wall of the upper part 91 and they are sealed.
  • the vessel 9 is filled with starting substances.
  • the vessel 9 further has two openings At a substantial height where the vessel has a maximum diameter, a duct 98 extends obliquely from the upper portion of the intermediate 92.
  • the duct 98 forms an acute angle to each of equator and tangent planes of the vessel 9 and the axis of the duct 98 is slightly inclined inwardly and upwardly in the interior direction of the vessel 9. In general, these angles are smaller than 30°.
  • the second opening is the end of the open bottom of the lower part 93 of the vessel 9.
  • a circulation passage comprising the pump 2, the mixing apparatus 1 and four conduits 4, 5, 6' and 7 is arranged between the lower part 93 and the inclined duct 98.
  • a closed circulation passage is formed through the pump 2, the vessel 9, withdrawal opening 8 and the conduits 4, 5, 6' and 7.
  • a water/hydrophobic liquid can be prepared without the aid of an emulsifier by using the device shown in Fig. 4 is described.
  • 9.5 l of distilled water is filled in the vessel 9 through the duct 97.
  • O.5 l of squalane is filled in the vessel 9 through the duct 95.
  • the ducts 95 and 97 are sealed.
  • the vessel 9 may be completely filled with water and squalane, or the upper part of the vessel 9 may be left vacant.
  • the pump 2 is started.
  • the flow direction is indicated by arrows in Fig. 4.
  • the same members as in the first embodiment are represented by the same reference numerals.
  • the third embodiment is different from the first embodiment mainly in that a jet pump 50 connected to the mixing apparatus 1 is arranged in the closed system.
  • a vessel 30 comprising a cover and ducts 31 and 32 is used.
  • the vessel 30 is filled with starting substances.
  • the vessel 30 is connected to the pump 2 through the conduit 6', withdrawal opening 8 and conduit 7 located at the lower portion of the vessel 30.
  • the flowout conduit 4 is connected to the inlet of the jet pump 50.
  • the internal structure of the jet pump 50 is shown in Fig. 6.
  • An inlet duct 54 of the jet pump 50 communicates with the vessel 30 through a duct 51.
  • the jet pump 50 exerts a function of promoting the mixing of two different liquids.
  • the jet pump 50 has a substantially cylindrical housing 52 having a hollow internal space, as shown in Fig. 6.
  • a nozzle 53 is inserted in the hollow internal space of the housing 52 and the top end of the nozzle 52 is connected to the duct 4.
  • a cylindrical space is formed in the vincinity of the top end of the nozzle 53 and an inlet duct 54 is inserted in the wall of the housing 52, and as the result, the hollow internal space of the inlet duct 54 communicates with the cylindrical space in the vincinity of the top end of the nozzle 53.
  • the water jet pump is used, but there may be adoped a method in which a branched pipe is used instead of the water jet pump and the outlet side of this tube is connected to the inlet side of the mixing apparatus 1.
  • the cock of the duct 31 is opened and the vessel 31 is filled with 9.5 l of ethyl alcohol. Then, the cock of the duct 32 is opened and O.5 l of squalane as the starting oil is filled in the vessel 30. The cock of the ducts 31 and 32 are closed.
  • a squalane-rich liquid in the vessel 30 is sucked into the pump 2 and is caused to flow in the vessel 30 through the conduit 4, jet pump 50, mixing apparatus 1 and conduit 5.
  • a closed system is formed.
  • an alcohol-rich liquid in the vessel 30 is injected into the jet pump 50 through the conduit 51. In this closed system, ethyl alcohol and squalane are mixed by the circulation. In this manner, a mixture of ethyl alcohol and squalane is formed.
  • the mixing apparatus 1 If the mixing apparatus 1 is used, at least two kinds of liquids can be stably and homogeneously mixed.
  • a laser beam source unit i.e., GL-803N, manufactured by Nakamura Rika Ko o K.K.
  • the cubic cell was set on a microscope (BH-2 manufactured by Olympus optical co., Ltd.) and a ultramicroscope was composed, together with the above-mentioned laser beam source unit.
  • the cubic cell was irradiated with a laser beam via the above-mentioned slit from the laser beam source unit.
  • the existence of oil drops was confirmed and the occurrence of a Brownian movement was also confirmed.
  • the resultant mixture was allowed to stand at room temperature for one day under a tightly sealed condition. As a result, it was confirmed that the water and the vitamin A oil in the vessel were separated and the underpositioned water was transparent and was not turbid. On the other hand, when one drop each of the upperpositioned vitamin A oil and the underpositioned water placed on a separate preparation was observed by the above-mentioned optical microscope, it was confirmed that neither the water drops nor the oil drops were a mixture of water and oil. Furthermore, neither oil in the water drops nor water in the oil drops were observed by the above-mentioned ultramicroscope.
  • the resultant mixtures were separated after allowing to stand at room temperature for one hour, into water and gas oil and the lower water phase was transparent.
  • the ethyl alcohol/vitamin A oil mixture prepared according to the first embodiment as the hydrophilic liquid/hydrophobic mixture was photographed by the microscope according to the above-mentioned method, it was confirmed that the droplet size of the vitamin A oil in ethyl alcohol was about 500 nm. No substantial change of the state was observed with respect to the distribution of ethyl alcohol and vitamin A oil between the mixture just after the mixing and the mixture which had been stored in a thermostat tank maintained at 50°C for 20 days.
  • the ethyl alcohol/vitamin A oil mixture on the preparation was warmed to evaporate water, adhesion of the oily substance onto the preparation was confirmed.
  • a plurality of mixing apparatuss 1 can be arranged in series or in parallel in one closed flow passage, and other substance can be supplied linearly or in the reversely rotated state in a vortex formed within the mixing apparatus. Furthermore, the mixing method, mixing device and mixture are not limited to those specifically disclosed in the examples.
  • hydrophobic liquid oily materials such as carnauba wax and liquid paraffin and fossil fuels such as benzene, decane, and gas oil, vegetable oils such as sesame oil, and by the term “hydrophilic liquid” are meant various alcohols such as monohydric and dihydric alcohols.
  • the obtained mixture is advantageous in the cost because an emulsifier need not be used, and hence, the limitations by the use of the emulsifier or the like are eliminated and the mixture can be widely used.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Colloid Chemistry (AREA)
  • Cosmetics (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Medicinal Preparation (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Polymerisation Methods In General (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Processing Of Solid Wastes (AREA)

Claims (5)

  1. Emulsion liquide exempte d'émulsifiant, comprenant au moins une phase de liquide hydrophobe choisi parmi le groupe composé de vitamine A, squalane, octane, cire carnauba, paraffine liquide, carburants fossiles, benzène, décane et huiles végétales et au moins une phase de liquide hydrophile choisi parmi le groupe composé d'eau et alcools monovalents, l'une desdites phases étant une phase dispersée de l'émulsion et ladite émulsion étant à l'état colloïdal stable, avec une grosseur de particules de la phase dispersée de 1.000 nm ou moins.
  2. Un procédé de production d'une émulsion liquide exempte d'émulsifiant à l'état colloïdal stable et composée d'au moins une phase de liquide hydrophobe et d'au moins une phase de liquide hydrophile à grosseur de particules de la phase dispersée de 1.000 nm ou moins, dans lequel les phases liquides sont circulées de manière répétée sous forme de leur mélange dans une chambre de mélange qui se compose d'une première partie et d'une seconde partie et qui est de forme axialement symétrique et dans laquelle le mélange est amené en circulation rotative autour de l'axe avec une composante de circulation parallèle à l'axe et dans laquelle la pression de circulation du mélange est réduite dans le sens de la circulation en élevant progressivement la vitesse de circulation du mélange jusqu'à la décharge coaxiale du mélange en rotation hors de la seconde partie de la chambre de mélange, la première partie de la chambre de mélange étant reliée à la seconde partie et présentant une partie supérieure opposée à la seconde partie, caractérisé en ce que la pression de circulation jusqu'à la décharge du mélange de la chambre de mélange est réduite à une pression minimale proche de la pression de vapeur du mélange, sans atteindre ou tomber au-dessous de la pression de vapeur, et que l'on fait circuler la majeure partie du mélange sous forme de fluide introduit dans la première partie de la chambre de mélange le long de la paroi intérieure de la première partie vers la partie supérieure, tout en continuant à être tourné, la circulation étant réfléchie à la partie supérieure et que la vitesse de circulation est progressivement élevée et qu'un état de vortex est formé sur l'axe central de la chambre de mélange vers la seconde partie.
  3. Un dispositif pour la mise en oeuvre du procédé suivant la revendication 2, comprenant un circuit de circulation et un mélangeur raccordé dans ladite boucle, le mélangeur (1) comprenant une chambre de mélange de forme symétrique en rotation dans un élément creux (14), avec une pluralité d'ouvertures d'entrée tangentielles (15) donnant dans une première partie de chambre reliée à une seconde partie de chambre de section conique dans le sens de la circulation et une sortie axiale étant coaxiale à l'axe de la chambre de mélange, caractérisé en ce que la première partie de chambre est en forme de paraboloïde rotatif du n-ième degré et que ladite seconde partie de chambre est en forme d'hyperboloïde inversé rotatif du n-ième degré, ladite sortie axiale étant une partie de conduit cylindrique (18), la paroi parabolique (14) de ladite première partie de chambre définissant une ligne focale tombant dans l'axe de rotation, lesdites ouvertures d'entrée (15) étant disposées sur une section large de la première partie de chambre qui est reliée à la seconde partie de chambre, à sa section la plus large, la somme des sections des ouvertures d'entrée (15) correspondant sensiblement à la section de ladite partie de conduit (18) et la différence entre ces sections étant de maximum 1:3, et qu'une chambre d'égalisation de pression (11) est prévue autour de ladite première partie de chambre, dans laquelle le mélange de fluides circule et passe par lesdites ouvertures d'entrée tangentielles (15) et qui est de forme cylindrique et coaxiale audit axe de rotation et comprend une paroi inférieure en amont de ladite première partie de chambre, un conduit d'entrée (16) définissant un angle aigu avec ledit axe donnant dans la chambre d'égalisation de pression (11) au centre de ladite paroi inférieure.
  4. Le dispositif suivant la revendication 3, caractérisé en ce que le degré de la fonction d'hyperboloïde définissant ledit segment conique correspond sensiblement au degré du paraboloïde définissant la première partie de chambre.
  5. Le dispositif suivant la revendication 3, comprenant un moyen de pompe dans ledit circuit de circulation, destiné à faire passer ledit fluide dans ladite chambre de mélange et à le faire circuler dans ledit circuit de circulation à un débit auquel la pression minimale créée à l'axe central est encore quelque peu supérieure à la pression de vapeur la plus élevée des éléments liquides à mélanger.
EP90906170A 1989-04-21 1990-04-20 Emulsion liquide sans emulsifiant; procede et dispositif pour la preparer Expired - Lifetime EP0469014B1 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE8905075U 1989-04-21
DE8905075U DE8905075U1 (fr) 1989-04-21 1989-04-21
JP103268/89 1989-04-22
JP10326889 1989-04-22
PCT/EP1990/000636 WO1990012639A1 (fr) 1989-04-21 1990-04-20 Emulsion liquide sans emulsifiant; procede et dispositif pour la preparer

Publications (2)

Publication Number Publication Date
EP0469014A1 EP0469014A1 (fr) 1992-02-05
EP0469014B1 true EP0469014B1 (fr) 1994-08-17

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EP90107576A Withdrawn EP0393715A1 (fr) 1989-04-21 1990-04-20 Emulsion liquide sans émulgateur et procédé et dispositif pour faire l'émulsion
EP90906170A Expired - Lifetime EP0469014B1 (fr) 1989-04-21 1990-04-20 Emulsion liquide sans emulsifiant; procede et dispositif pour la preparer

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EP90107576A Withdrawn EP0393715A1 (fr) 1989-04-21 1990-04-20 Emulsion liquide sans émulgateur et procédé et dispositif pour faire l'émulsion

Country Status (13)

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EP (2) EP0393715A1 (fr)
AT (1) ATE110001T1 (fr)
AU (1) AU5422990A (fr)
CA (1) CA2051438A1 (fr)
DD (1) DD299620A5 (fr)
DE (1) DE69011679T2 (fr)
DK (1) DK0469014T3 (fr)
ES (1) ES2057555T3 (fr)
HU (1) HUT61909A (fr)
IL (1) IL94162A (fr)
PT (1) PT93846A (fr)
RU (1) RU2072891C1 (fr)
WO (1) WO1990012639A1 (fr)

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DE9103927U1 (fr) * 1991-03-30 1991-07-25 Oswald Bender Gmbh, 6233 Kelkheim, De
US7810674B2 (en) 2005-07-26 2010-10-12 Millipore Corporation Liquid dispensing system with enhanced mixing
US7950547B2 (en) 2006-01-12 2011-05-31 Millipore Corporation Reservoir for liquid dispensing system with enhanced mixing
DE102007047478A1 (de) * 2007-09-27 2009-04-16 Charité - Universitätsmedizin Berlin Vorrichtung und Verfahren zur gleichmäßigen Verteilung von Mikropartikeln in einer Flüssigkeit
RU2463100C1 (ru) * 2011-03-05 2012-10-10 Овченкова Оксана Анатольевна Способ проведения реакций и реактор для его осуществления
RU2486950C1 (ru) * 2012-03-27 2013-07-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Пензенская государственная технологическая академия" Способ получения растворов в цилиндрической вертикальной емкости, нагреваемой в основном со стороны днища, например, для работы шлихтовальной машины ткацкого производства

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR844009A (fr) * 1938-04-14 1939-07-18 Préparation d'émulsions et de suspensions colloïdales dans l'eau, de parfums, essences aromatiques, huiles de vaseline et autres produits utilisés en parfumerie, en pharmacie et dans l'industrie
FR2461515A1 (fr) * 1979-07-24 1981-02-06 Robert Guerin Dispositif de traitement d'au moins deux fluides comprenant un liquide, notamment pour la realisation d'emulsion de deux liquides non solubles l'un dans l'autre
AU541324B2 (en) * 1979-08-01 1985-01-03 Exxon Research And Engineering Company Emulsifying immiscible liquids
DE3028005A1 (de) * 1980-07-24 1982-02-18 Bayer Ag, 5090 Leverkusen Verfahren zur herstellung von pharmazeitischen und kosemtischen dispersionen
GB2092025A (en) * 1981-01-30 1982-08-11 Ici Plc Spraying emulsions
US4430251A (en) * 1981-09-29 1984-02-07 Hoffert Manufacturing Co., Inc. High energy emulsifier
EP0263443B1 (fr) * 1986-10-08 1992-05-20 Zugol AG Procédé et dispositif pour produire une émulsion eau-en-huile
EP0312642A1 (fr) * 1987-10-23 1989-04-26 "Harrier" Gmbh Gesellschaft Für Den Vertrieb Medizinischer Und Technischer Geräte Procédé pour introduire du gaz dans de l'eau en quantité au-dessus de l'équilibre, appareil pour exécuter le procédé et eau obtenue à partir de ce procédé

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PT93846A (pt) 1990-11-20
EP0469014A1 (fr) 1992-02-05
RU2072891C1 (ru) 1997-02-10
DK0469014T3 (da) 1994-09-19
ATE110001T1 (de) 1994-09-15
AU5422990A (en) 1990-11-16
DD299620A5 (de) 1992-04-30
WO1990012639A1 (fr) 1990-11-01
DE69011679D1 (de) 1994-09-22
CA2051438A1 (fr) 1990-10-22
DE69011679T2 (de) 1995-02-16
IL94162A0 (en) 1991-01-31
HUT61909A (en) 1993-03-29
IL94162A (en) 1995-08-31
EP0393715A1 (fr) 1990-10-24
HU903661D0 (en) 1991-12-30
ES2057555T3 (es) 1994-10-16

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